CN104849297A - Method for authenticating oxidizing/reducing functional groups in water-soluble organic matters - Google Patents
Method for authenticating oxidizing/reducing functional groups in water-soluble organic matters Download PDFInfo
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- CN104849297A CN104849297A CN201510250467.6A CN201510250467A CN104849297A CN 104849297 A CN104849297 A CN 104849297A CN 201510250467 A CN201510250467 A CN 201510250467A CN 104849297 A CN104849297 A CN 104849297A
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Abstract
The invention relates to a method for authenticating oxidizing/reducing functional groups in water-soluble organic matters. The method comprises the following steps that (A) samples are prepared and are subjected to structure analysis; (B) a DMSO (dimethylsulfoxide) solution containing the water-soluble organic matters is prepared; (C) a water-soluble organic matter oxidizing/reducing curve is measured; (D) functional groups with the oxidization capability in the water-soluble organic matters are determined; (E) functional groups with reducing capability in the water-soluble organic matters are determined. When the method provided by the invention is adopted for measuring the oxidizing/reducing functional groups in the water-soluble organic matters, the sample demand is low, the analysis is fast and convenient, and the analysis result is precise and comprehensive.
Description
Technical field
The invention belongs to Environmental Analytical Chemistry field, be specifically related to the assay method of oxidation/reduction ability functional group in a kind of organism.
Background technology
In environment, water soluble organic substance has various functions, and it can provide C, N nutriment for microorganism, absorption and coordination heavy metal, and solubilisation of hydrophobic contact scar thing, causes the change at its biological effectiveness and environment home to return to; In addition, water soluble organic substance as electron shuttle body, can also obtain or lose electronics, has oxidation and restoring function.The oxidation/reduction ability of water soluble organic substance can accelerate the conversion of heavy metal and the degraded of organic pollutant, has important environmental effect.
The oxidation/reduction performance measuring water soluble organic substance has multiple method, wherein, cyclic voltammetry in electrochemical method is the most quick and convenient, directly can show the oxidation/reduction performance of water soluble organic substance, water is the most frequently used solvent of water soluble organic substance, but the easy electrolysis of the water capacity, its reduction peak may be overlapping with the reduction peak of water soluble organic substance, affect the analysis of water soluble organic substance oxidation/reduction performance, therefore, the oxidation/reduction performance of cyclic voltammetry water soluble organic substance, needs to eliminate water mitigation.
The mensuration of oxidation/reduction functional group in water soluble organic substance, method the most frequently used at present measures its oxidation/reduction ability, correlation analysis is carried out again with organic various structural parameters, and then determine that those organism have oxidation and restoring function, but, said method needs the oxidation/reduction ability of water soluble organic substance and structure composition parameter to carry out quantization signifying, this not only needs a large amount of time, more troublesomely be, some organic structural parameters, as FFIR data, sxemiquantitative can only be carried out, can not entirely quantitatively calculate, to determine in water soluble organic substance that those functional groups have oxidation/reduction performance bring difficulty to above-mentioned.
Summary of the invention
The object of the present invention is to provide a kind of method identifying oxidation/reduction functional group in water soluble organic substance, by analyzing the correlativity of oxidation/reduction curve and its structural characterization spectral line in water soluble organic substance, and then determine functional group and the oxidation/reduction ability thereof in water soluble organic substance with oxidation/reduction ability.
To achieve these goals, the method for oxidation/reduction functional group in qualification water soluble organic substance provided by the invention, key step is:
A) preparation of water soluble organic substance and structure analysis: extract water soluble organic substance and carry out freeze drying and make pressed powder, adopt solid-state
13c nuclear magnetic resonance or Fourier transformation infrared spectrometer, the nuclear magnetic resonance of working sample or infrared spectrogram also by statistical conversion, obtain organic constitution information data.
B) the organic DMSO solution preparation of containing water-soluble: water soluble organic substance pressed powder is dissolved in containing NaClO
4ultrapure water in, adopt chromatographically pure DMSO by above-mentioned solution dilution to 100 times or more subsequently, obtained DMSO solution.
C) water soluble organic substance redox (CV) curved scanning: carry out negative sweeping to the organic DMSO solution of containing water-soluble on electrochemical workstation, be swept to-2V from 0V, must contain the CV1 curve of reduction peak; Scan rear cleaning electrode, again got the organic DMSO solution of containing water-soluble and just sweep, be also swept to-2V from 0V, the CV2 curve of oxidation peak must have been contained.
D) there is the determination of oxidability functional group: after CV1 curve data is multiplied by negative 1 in water soluble organic substance, Two-dimensional Correlation Analysis is carried out again with nuclear magnetic resonance figure or infared spectrum data, corresponding functional group is the functional group with oxidability with CV1 curve positive correlation spectral band, positive correlation coefficient is higher, nuclear magnetic resonance or the functional group's oxidability corresponding to ir data stronger.
E) there is in water soluble organic substance the determination of reducing power functional group: CV2 curve data and nuclear magnetic resonance figure or infared spectrum data are carried out Two-dimensional Correlation Analysis, the functional group corresponding with CV2 curve data positive correlation collection of illustrative plates is the functional group with reducing power, positive correlation coefficient is higher, nuclear magnetic resonance or functional group's reducing power corresponding to ir data stronger.
In described method, in steps A, the quantity of sample is no less than 5.
The organism of the water soluble organic substance that in described method, the sample in steps A can be compost, landfill waste, soil extract obtain or lake, river and groundwater resources.
In described method, in steps A, water soluble organic substance needs through desalting and removing metal ion treatment.
In described method, NaClO in step B
4for top grade is pure.
In described method, in step BDMSO solution, water soluble organic substance sample concentration is higher than 50mg/L.
In described method, in step C and D, auxiliary electrode is Pt electrode, and contrast electrode is Ag/AgCl electrode, sweep speed 1050mV/s, and sensitivity is 10
-5~ 10
-6a.
Advantage of the present invention is as follows:
1, analyze fast, sample requirements is few.Adopt the oxidation/reduction functional group in the method determination water soluble organic substance, owing to decreasing a lot of analytical procedure than classic method, and be microchemical analysis, therefore, this analytical approach not only sample requirements is few, and analyzes quick.
2, result comprehensively and accurately.Owing to adopting the Two-dimensional Correlation Analysis correlativity of all organic constitution parameters and its oxidation/reduction performance, therefore can provide functional group's information with oxidation/reduction performance comprehensively.In addition, can judge the size of oxidation operation/reducing power according to association's related coefficient size, therefore this analytical approach precision is high.
Accompanying drawing explanation
Fig. 1 is the techniqueflow chart of oxidation/reduction performance functional group in qualification water soluble organic substance;
In Fig. 2, a, c are oxidation operations/go back virgin curve, and b, d are the two-dimensional correlation figure with infrared spectrum.
Embodiment
Below in conjunction with accompanying drawing, the specific embodiment of the present invention is described.
Sample preparation and structure analysis: 6, the sample gathering different composting period, be numbered C0, C7, C14, C21, C28, C51, extract humic acid, by humic acid freeze drying after desalination and duplicate removal metal, adopt Fourier transformation infrared spectrometer working sample infrared spectrogram and data are derived with absorption spectrum form.
The preparation of Humic Acid Solution: the humic acid solid sample obtained by extraction purification is dissolved in containing NaClO
4ultrapure water in, adopt chromatographically pure DMSO to dilute 100 times subsequently, obtain the DMSO solution that humic acid concentration is greater than 200mg (C)/L.
Humic Acid Solution cyclic voltammetric (CV) curved scanning: adopt the oxidation/reduction performance of electrochemical workstation to humic acid to measure, scanning auxiliary electrode used is Pt electrode, contrast electrode is Ag/AgCl electrode, sweep speed 50mV/s, and sensitivity is 10
-6a.First be negative sweeping, be swept to-2V from 0V, the CV1 curve of reduction peak must be contained, as shown in Figure 2 a, near-1.0V, occurred reduction peak; Scanned rear cleaning electrode, water-soluble organic solution is just swept again, is also swept to-2V from 0V, must contain the CV2 curve of oxidation peak, as shown in Figure 2 c, occur oxidation peak near-0.25V.
There is the determination of the functional group of oxidability: after CV1 curve data is multiplied by negative 1 in Humic Acid Solution, Two-dimensional Correlation Analysis is carried out again with the infared spectrum data of humic acid sample, gained correlogram as shown in Figure 2 b, the reduction peak in this figure near-1.0V and 1463cm
-1(carboxylic acid), 1631cm
-1(C=C functional group), 3408cm
-1the infrared spectrum positive correlation of (phenolic hydroxyl group, carboxylic acid) wave band, its positive correlation coefficient reduces successively, in display humic acid, phenolic hydroxyl group, carboxylic acid and C=C functional group have oxidability, and its oxidability power is carboxylic acid >C=C unsaturated link > phenolic hydroxyl group.
There is in humic acid the determination of the functional group of reducing power: the infared spectrum data of humic acid sample and CV2 curve data are carried out Two-dimensional Correlation Analysis, analysis result as shown in Figure 2 d, the oxidation peak in this figure near-0.25V and 1463cm
-1(carboxylic acid), 1631cm
-1(C=C functional group), 3408cm
-1the infrared spectrum positive correlation of (phenolic hydroxyl group, carboxylic acid) wave band, its positive correlation coefficient reduces successively, in display humic acid, phenolic hydroxyl group, carboxylic acid and C=C functional group have reducing power, and its reducing power power is carboxylic acid >C=C unsaturated link > phenolic hydroxyl group.
Claims (8)
1. identify a method for oxidation/reduction functional group in water soluble organic substance, its key step is:
A) water soluble organic substance preparation and structure analysis: the water soluble organic substance in extraction environment medium also carries out purifying and freeze drying, adopts solid-state
13c nuclear magnetic resonance or Fourier transformation infrared spectrometer, the nuclear magnetic resonance of working sample or infrared spectrogram also by statistical conversion, obtain organic constitution information data;
B) the organic DMSO solution preparation of containing water-soluble: water soluble organic substance solid sample is dissolved in containing NaClO
4ultrapure water in, dilute above-mentioned solution more than 100 times with DMSO, the obtained organic DMSO solution of containing water-soluble;
C) water soluble organic substance redox curved scanning: carry out negative sweeping to the organic DMSO solution of containing water-soluble on electrochemical workstation, be swept to-2V from 0V, must contain the CV1 curve of reduction peak; Scan rear cleaning electrode, again got the organic DMSO solution of containing water-soluble and just sweep, be also swept to-2V from 0V, the CV2 curve of oxidation peak must have been contained;
D) there is the determination of the functional group of oxidability: after curve C V1 data are multiplied by negative 1 in water soluble organic substance, Two-dimensional Correlation Analysis is carried out again with steps A gained nuclear magnetic resonance or infared spectrum data, the functional group corresponding with the positively related spectral band of CV1 curve data is the functional group with oxidability, positive correlation coefficient is higher, nuclear magnetic resonance or the functional group's oxidability corresponding to ir data stronger;
E) there is in water soluble organic substance the determination of the functional group of reducing power: curve C V2 data and steps A gained nuclear magnetic resonance or infared spectrum data are carried out Two-dimensional Correlation Analysis, the functional group corresponding with the positively related collection of illustrative plates of CV2 curve data is the functional group with reducing power, positive correlation coefficient is higher, nuclear magnetic resonance or functional group's reducing power corresponding to ir data stronger.
2. method according to claim 1, wherein, in steps A, the quantity of sample is no less than 5.
3. method according to claim 1, the organism of the water soluble organic substance that wherein, the sample in steps A is compost, landfill waste, soil extract obtain or lake, river and groundwater resources.
4. method according to claim 1, wherein, the water soluble organic substance that steps A obtains is through desalting and removing metal ion treatment.
5. method according to claim 1, wherein, the DMSO in step B is chromatographically pure.
6. method according to claim 1, wherein, the NaClO in step B
4for top grade is pure.
7. method according to claim 1, wherein, in step B, in DMSO solution, the concentration of water soluble organic substance is not less than 50mg/L.
8. method according to claim 1, wherein, in step C, auxiliary electrode is Pt electrode, and contrast electrode is Ag/AgCl electrode, sweep speed 1050mV/s, and sensitivity is 10
-5~ 10
-6a.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109758782A (en) * | 2019-01-30 | 2019-05-17 | 中国环境科学研究院 | A kind of quick method for extracting compost water soluble organic substance |
| CN110057774A (en) * | 2019-05-17 | 2019-07-26 | 中国科学院南京地理与湖泊研究所 | A method of based on total organic carbon in infrared spectroscopy fast quantification lacustrine deposit |
| CN112945899A (en) * | 2021-01-29 | 2021-06-11 | 燕山大学 | Method for identifying polyglutamic acid compound fertilizer |
-
2015
- 2015-05-15 CN CN201510250467.6A patent/CN104849297A/en active Pending
Non-Patent Citations (2)
| Title |
|---|
| WOLFGANG KAIMA，JAN FIEDLERB: "Spectroelectrochemistry: the best of two worlds", 《CHEM. SOC. REV.》 * |
| 郑华均,马淳安: "光谱电化学原位测试技术的应用及进展", 《浙江工业大学学报》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109758782A (en) * | 2019-01-30 | 2019-05-17 | 中国环境科学研究院 | A kind of quick method for extracting compost water soluble organic substance |
| CN110057774A (en) * | 2019-05-17 | 2019-07-26 | 中国科学院南京地理与湖泊研究所 | A method of based on total organic carbon in infrared spectroscopy fast quantification lacustrine deposit |
| CN110057774B (en) * | 2019-05-17 | 2020-06-12 | 中国科学院南京地理与湖泊研究所 | Method for rapidly quantifying total organic carbon in lake deposition based on infrared spectrum |
| CN112945899A (en) * | 2021-01-29 | 2021-06-11 | 燕山大学 | Method for identifying polyglutamic acid compound fertilizer |
| CN112945899B (en) * | 2021-01-29 | 2022-10-14 | 燕山大学 | Method for identifying polyglutamic acid compound fertilizer |
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